CN102230917A - Analyzing device using gas phase chromatography and inverse gas phase chromatography together - Google Patents
Analyzing device using gas phase chromatography and inverse gas phase chromatography together Download PDFInfo
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- CN102230917A CN102230917A CN2011100893169A CN201110089316A CN102230917A CN 102230917 A CN102230917 A CN 102230917A CN 2011100893169 A CN2011100893169 A CN 2011100893169A CN 201110089316 A CN201110089316 A CN 201110089316A CN 102230917 A CN102230917 A CN 102230917A
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Abstract
The invention discloses an analyzing device using gas phase chromatography and inverse gas phase chromatography together. The analyzing device comprises a gas phase chromatographic column and an inverse gas phase chromatographic column, wherein the input end of the gas phase chromatographic column is connected with a sample injector; the output end of the gas phase chromatographic column is connected with the input end of the inverse gas phase chromatographic column; the output end of the gas phase chromatographic column is further connected with a first detector; the input end of the inverse gas phase chromatographic column is further connected with a gas carrying pipe; the output end of the inverse gas phase chromatographic column is connected with a second detector; and the first detector and the second detector are both connected with a signal acquisition device. Due to the adoption of the analyzing device, the adsorption performance of a detected solid adsorption material on different single probes can be inspected, the adsorption performance of different solid adsorption materials on different components in a mixed probe can be inspected simultaneously, and the developing efficiency of an inverse gas phase chromatography technology is increased.
Description
Technical field
The present invention relates to a kind of device of testing solid material surface character, particularly a kind of gas chromatography-anti-gas chromatography combined analysis device.
Background technology
In in the past to solid material surface performance evaluation process, often use technology such as scanning electron microscope, X-ray energy spectrum by surface naturies such as the specific surface area of adsorbent itself and pore volume are measured, but these methods can not reflect the interaction ability between the probe of solid material surface and its effect, especially are difficult to investigate solid material to the interaction between the different component material in the mixed probe.Traditional anti-gas chromatography mainly is to insert in the packed column by institute is surveyed solid material, makes it pass through this packed column after will vaporizing with single probe molecule of its effect.Like this, when this probe molecule by by the packed column of different kinds material the time, will produce different relative retention times, according to relative retention time value and some other chromatographic parameter can investigate this probe molecule with measure and monitor the growth of standing timber and expect interaction between the surface.But classic method is for the test of some sorbing materials, tend to cause probe molecule to pass through the difficult calculating of sorbing material surface relative retention time, particularly for mixed probe, traditional anti-gas chromatography is difficult to its separation, thereby causing the inseparable problem of each composition can occur behind the peak, so just need when test, standard model be arranged and strengthen the difficulty of test, be unfavorable for test at different components in the mixed probe.
Summary of the invention
Problem to be solved by this invention provides a kind of gas chromatography-anti-gas chromatography combined analysis device, overcomes the above-mentioned problems in the prior art.
Gas chromatography of the present invention-anti-gas chromatography combined analysis device, comprise a gas chromatographic column and an anti-gas chromatographic column, the input end of described gas chromatographic column is connected with an injector, the output terminal of gas chromatographic column is connected with the input end of described anti-gas chromatographic column, the output terminal of gas chromatographic column also is connected with first detecting device, the input end of described anti-gas chromatographic column also is connected with a carrier gas pipe, the output terminal of anti-gas chromatographic column is connected with second detecting device, and described first detecting device, second detecting device all are connected with a signal collector.
Be connected by the insulation pipeline between the output terminal of gas chromatographic column of the present invention and the input end of described anti-gas chromatographic column.
Gas chromatographic column of the present invention is a capillary column.
Anti-gas chromatographic column of the present invention is a packed column.
Carrier gas pipe of the present invention is provided with flow control valve.
Be connected by a four-way valve between the input end of the output terminal of gas chromatographic column of the present invention, first detecting device, anti-gas chromatographic column and the carrier gas pipe.
By above technical scheme, gas chromatography of the present invention-anti-gas chromatography combined analysis device, adopt anti-gas chromatography principle to measure under the design temperature different probe molecule, as coefficient of diffusion, all kinds of crystallization parameters in adsorbent of surface adsorption enthalpy, surface acid alkalescence, surface compatability, probe molecule, the otherness that detects different batches sample surfaces chemical property, the surface heterogeneous medium (by the distribution of survey surface energy position) of measuring single composition or multicomponent mixture, the glass transition temperature of the block object of measurement etc. in the interaction of surveys solid surface.This device both can investigate the solid adsorption material of surveying to the absorption property of the single probe of difference, can investigate the absorption property of different solid adsorption materials simultaneously again to different components in the mixed probe, realized simultaneously the interaction force between measure and monitor the growth of standing timber material surface and the different probe molecule being analyzed, this will increase the dirigibility of systems approach greatly, original analytical approach be had the effect that promotes and optimize.
Description of drawings
Fig. 1 is the structural drawing of gas chromatography of the present invention-anti-gas chromatography combined analysis device.
Among the figure, the 1----injector; The 2----flow control valve; The 3----gas chromatographic column; The 4----four-way valve; 5----is incubated pipeline; The anti-gas chromatographic column of 6----; 7----first detecting device; 8----second detecting device; The 9----signal collector.
Embodiment
As shown in Figure 1, gas chromatography of the present invention-anti-gas chromatography combined analysis device, comprise a gas chromatographic column 3 and an anti-gas chromatographic column 6, the input end of gas chromatographic column 3 is connected with an injector 1, the output terminal of gas chromatographic column 3 is connected with the input end of anti-gas chromatographic column 6, the output terminal of gas chromatographic column 3 also is connected with first detecting device 7, the input end of anti-gas chromatographic column 6 also is connected with a carrier gas pipe, the output terminal of anti-gas chromatographic column 6 is connected with second detecting device 8, first detecting device 7, second detecting device 8 all is connected with a signal collector 9.
Be connected by insulation pipeline 5 between the output terminal of gas chromatographic column and the input end of anti-gas chromatographic column, guarantee the temperature between the probe operation.
Be connected by four-way valve 4 between the input end of the output terminal of gas chromatographic column 3, first detecting device 7, anti-gas chromatographic column 6 and the carrier gas pipe, and the carrier gas pipe is provided with flow control valve 2, can regulates the carrier gas input quantity of carrier gas pipe.First detecting device 7 and second detecting device 8 can be thermal conductivity cell detector (TCD), also can be hydrogen flame ionization detector (FID).
This device can adopt gas direct injected or micro liquid sample introduction, for example adopt headspace sampling or with the liquid probe molecule that will test vaporize the back sample introduction.Gas chromatographic column 3 adopts capillary column, and anti-gas chromatographic column 4 adopts packed column.Probe molecule after being vaporized is at first by after capillary column (can the select suitable capillary column according to the actual requirements) temperature programme separating it.Separate the back and enter first detecting device 7 from the sample shunting back part that capillary column flows out and detect, another part enters second detecting device 8 after by packed column and detects.
The input end that this device is provided with anti-gas chromatographic column 3 also is connected with a carrier gas pipe, make one tunnel carrier gas pass through packed column with the sample that kapillary flows out, therefore avoided when the capillary column carrier gas flux is restricted, and be affected by the carrier gas flux of packed column.Additional one tunnel carrier gas will reduce requirement to the gas-phase chromatographic capillary column internal diameter by packed column beyond the capillary column, and appropriate design is by the carrier gas flux of packed column, thus the feasible science, more flexible more of testing.
This device adopts dual-detector to detect simultaneously, determine the relative retention time of probe molecule by investigating probe molecule appearance time difference on two detecting devices, and then the interaction of different probe molecule and institute's survey storeroom and the surface nature of the material of measuring and monitoring the growth of standing timber are tested by material in the packed column.
This device can be implemented in the test mixing probe with the institute measure and monitor the growth of standing timber the material surface interaction before, at first make mixed probe obtain separating by gas chromatographic column, so just can effectively avoid mixing the gas phase probe directly by behind the anti-gas chromatographic column, gas chromatography exists the peak to be difficult to problem separately.This will improve the problem that the classical inverse gas chromatography system can only be measured at single probe to a great extent, simplify operation.This device has been realized the coupling of gas chromatography and anti-gas chromatography, farthest brought into play the function of gas chromatography separate probe molecule, make systems approach more scientific and reasonable, it is more convenient to detect, especially test becomes possibility to make in the mixed probe different components and solid material surface interact simultaneously, and this also will simplify the mensuration process of other surface nature of solid material greatly.
During mensuration, at first mixed probe molecule different components is separated preferably, will effectively avoid mixing in the classical inverse gas phase chromatographic device test gas phase probe like this and directly go out the peak behind the packed column by strong absorption property material and be difficult to problem separately by gas chromatographic column 3.Then, its surface nature is investigated by the difference of the ratio retention time of survey sorbing material by different components in the mixed probe, thus the interaction of the interaction of probe molecule more of the same race and different solid material surfaces or different probe molecule and same solid material surface and further determine other surface nature that institute measures and monitor the growth of standing timber and expects by these tests.
A specific embodiment of the present invention is: above-mentioned injector adopts the carousel-type automatic sampler, Agilent 6890N gas chromatograph, and the capillary column model is CP-Poraplot-Q, long 27.5m, internal diameter 0.53mm; Anti-gas chromatographic column adopts packed column, the about 2mm of packed column internal diameter, and the about 6mm of external diameter is about 8cm.200 ℃ of column temperatures, carrier gas flux 26.5mL/min, sample size are that 0.2 μ l, injection port split ratio are that 30: 1,250 ℃ of injector temperatures, detecting device are fid detector and TCD detecting device, and temperature is 250 ℃.Do following experiment below, all fill 16mg institute test sample product in the packed column, and selected for use acetaldehyde, acetone, butyraldehyde, benzene, phenixin, tetrahydrofuran, ethyl acetate, test their absorption properties on survey solid adsorption material surface as probe molecule.
During experiment, at first be installed to ready packed column on the gas chromatograph of adjusting and guarantee impermeability, adjust carrier gas flux.Carry out the aging of anti-gas chromatographic column with the gas flow method, be about to anti-gas chromatographic column inlet end and link to each other endpiece emptying with the outlet of gas chromatograph vaporizer.Feed carrier gas (flow velocity is 10.5mL/min) half an hour, air in the system is driven away.The rising chromatogram column temperature is controlled at about 200 ℃ and wore out 2 hours.After wearing out well, connect the detecting device inspection, obtain baseline stably.
Solid material is as follows to the computing method of the adsorption free energy Δ G of probe molecule:
ΔG＝-RTInVg+K (1)
In the following formula, Δ G is standard adsorption free energy (J/mol); R is universal gas constant 8.3145J/ (molK); T is absolute temperature (K); The K value is relevant with amount, surface area and the adsorbed state of polymkeric substance, so K is constant (J/mol) in same chromatographic column.
Specific retention volume Vg can obtain by following formula:
In the formula, Δ t=t
r-t
0, t
r, t
0It is respectively the retention time (s) and the dead time (s) of probe molecule; F is the flow rate of carrier gas (mL/s) of anti-gas chromatography column outlet; M is the quality (g) of stationary phase; T is environment temperature (K); P
iAnd P
0Be respectively anti-gas chromatographic column import and outlet pressure (Pa); Vg is specific retention volume (mL/g).
Embodiment 1-7 is that the A material of surveying is investigated the different probe absorption property, obtains a result as follows according to following formula (1) and (2):
During 200 ℃ of table 1 A solid materials different gas phase probe absorption properties are investigated
| Embodiment | Institute's test sample product name of an article | ΔG，kJ/mol |
| 1 | The A material is investigated the acetaldehyde adsorption free energy | -19.4651 |
| 2 | The A material is investigated the acetone adsorption free energy | -24.9012 |
| 3 | The A material is investigated the butyraldehyde adsorption free energy | -28.8257 |
| 4 | The A material is investigated the benzene adsorption free energy | -38.489 |
| 5 | The A material is investigated the ethyl acetate adsorption free energy | -31.9238 |
| 6 | The A material is investigated the tetrahydrofuran adsorption free energy | -28.1969 |
| 7 | The A material is investigated the phenixin adsorption free energy | -30.832 |
From above embodiment result as can be seen, the A solid adsorption material has certain difference to different gas phase probe absorption properties, so this method can be estimated sorbing material preferably to the absorption property of different probe molecule.
The A solid material surface is as follows to the computing method of different probe adsorption enthalpy Δ H and entropy Δ S:
Can draw according to thermodynamics formula Δ G=Δ H-T Δ S and above-mentioned formula (1):
-RTInVg＝ΔH-TΔS (3)
Thereby draw:
In the formula: Vg is specific retention volume (mL/g), and R is universal gas constant 8.3145J/ (molK), and T is environment temperature (K).
By--InVg maps to 1/T, can obtain adsorption enthalpy and the entropy of institute's test sample product to different probe from the slope and the intercept of the straight line of gained.
Embodiment 8-12 is that the A solid material detects different gas phase composition surface adsorption enthalpys such as acetone, ethanol, tetrahydrofuran, phenixin, ethyl acetate, obtains a result as follows according to following formula (4):
Table 2.A solid material is to different gas phase composition surface adsorption enthalpys
| Embodiment | Institute's test sample product name of an article | ΔH，kJ/mol |
| 8 | The A material is investigated acetone surface adsorption enthalpy | -47.055 |
| 9 | The A material is investigated ethanol carbon surface adsorption enthalpy | -37.141 |
| 10 | The A material is investigated tetrahydrofuran surface adsorption enthalpy | -53.081 |
| 11 | The A material is investigated phenixin surface adsorption enthalpy | -53.307 |
| 12 | The A material is investigated ethyl acetate surface adsorption enthalpy | -62.666 |
According to the acid-base theory of Gutmann, the probe molecule A material surface adsorption enthalpy Δ H in conjunction with said method records, can calculate its surperficial acidity constant and alkaline constant with the following method:
-ΔH＝K
a×DN+K
b×AN (5)
In the formula, DN, AN are respectively the electron donor constant and the electron accepter constant of the polarity probes molecule of Gutmann definition, and Ka, Kb are respectively the acidity constant and the alkaline constant of adsorbent surface.By the various polarity probe-Δ H/AN maps to DN/AN, from the slope of the straight line of gained and semiquantitative Ka constant and the Kb constant that intercept can obtain adsorbent surface soda acid character.
Embodiment 13-15 is an A solid material surface Acidity of Aikalinity test result, obtains a result as follows according to following formula (5):
Table 3.A solid material surface Acidity of Aikalinity test result
| Embodiment | Institute's test sample product name of an article | |
| 13 | A material surface acidity constant Ka | 2.3612 |
| 14 | A material surface alkalescence constant K b | 1.2206 |
| 15 | Ka/Kb | 1.9344 |
From embodiment 13-15 as can be seen, the soda acid constant ratio of A material is greater than 1, so show than highly acid.
Claims (6)
1. gas chromatography-anti-gas chromatography combined analysis device, comprise a gas chromatographic column and an anti-gas chromatographic column, it is characterized in that, the input end of described gas chromatographic column is connected with an injector, the output terminal of gas chromatographic column is connected with the input end of described anti-gas chromatographic column, the output terminal of gas chromatographic column also is connected with first detecting device, the input end of described anti-gas chromatographic column also is connected with a carrier gas pipe, the output terminal of anti-gas chromatographic column is connected with second detecting device, described first detecting device, second detecting device all is connected with a signal collector.
2. gas chromatography according to claim 1-anti-gas chromatography combined analysis device is characterized in that, is connected by the insulation pipeline between the output terminal of described gas chromatographic column and the input end of described anti-gas chromatographic column.
3. gas chromatography according to claim 1-anti-gas chromatography combined analysis device is characterized in that, described gas chromatographic column is a capillary column.
4. gas chromatography according to claim 1-anti-gas chromatography combined analysis device is characterized in that, described anti-gas chromatographic column is a packed column.
5. gas chromatography according to claim 1-anti-gas chromatography combined analysis device is characterized in that, described carrier gas pipe is provided with flow control valve.
6. gas chromatography according to claim 1-anti-gas chromatography combined analysis device is characterized in that, is connected by a four-way valve between the input end of the output terminal of described gas chromatographic column, first detecting device, anti-gas chromatographic column and the carrier gas pipe.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110089316.9A CN102230917B (en) | 2011-04-11 | 2011-04-11 | Analyzing device using gas phase chromatography and inverse gas phase chromatography together |
| PCT/CN2011/077205 WO2012139340A1 (en) | 2011-04-11 | 2011-07-15 | Gas chromatography-inverse gas chromatography coupled analysis device |
| US13/809,586 US8943872B2 (en) | 2011-04-11 | 2011-07-15 | Gas chromatography—inverse gas chromatography combined analysis device |
| JP2013509443A JP5250164B2 (en) | 2011-04-11 | 2011-07-15 | Analytical instrument using both gas chromatography and inverse gas chromatography |
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| CN102590389A (en) * | 2012-02-27 | 2012-07-18 | 上海烟草集团有限责任公司 | Gas phase chromatograph with dual detectors |
| CN102735776A (en) * | 2012-07-03 | 2012-10-17 | 中昊晨光化工研究院 | Gas chromatographic separation system and application thereof, and method for detecting trace impurities in tetrafluoroethylene |
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| CN204027852U (en) * | 2011-01-18 | 2014-12-17 | 魄金莱默保健科学有限公司 | Sampling system, steam sampling system, sampler, gas chromatography system and external member |
| CN103471958B (en) * | 2013-09-25 | 2015-11-18 | 上海烟草集团有限责任公司 | Full-automatic tobacco dynamic water analyzes climate box |
| TWI679274B (en) * | 2014-12-05 | 2019-12-11 | 德商格雷氏公司 | Process for evaluating the catalytic performance of a porous solid |
| JP7275948B2 (en) * | 2019-07-11 | 2023-05-18 | 株式会社島津製作所 | Analysis equipment |
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| US20030108448A1 (en) * | 2001-12-10 | 2003-06-12 | Sacks Richard Douglas | Pulsed carrier gas flow modulation for selectivity enhancements with gas chromatography using series-coupled column ensembles |
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| JPS5643566A (en) * | 1979-09-17 | 1981-04-22 | Mitsubishi Electric Corp | Insulation life estimating method of electrical machinery |
| US4962042A (en) * | 1988-05-25 | 1990-10-09 | The Dow Chemical Company | Method for on-column injection gas chromatography |
| US6134945A (en) * | 1997-12-18 | 2000-10-24 | Gerstel Gmbh | Method for applying samples to be analyzed by gas chromatography and sampling tube |
| GB2342870A (en) * | 1998-10-23 | 2000-04-26 | Surface Measurement Systems Lt | Inverse chromatography |
| CN101206206A (en) * | 2006-12-19 | 2008-06-25 | 中国药品生物制品检定所 | Method for detecting residual solvent in medicine |
| US7803635B1 (en) * | 2008-02-27 | 2010-09-28 | EST Analytical, Inc | Purge and trap concentrator with sparge vessel |
| CN201637726U (en) * | 2009-12-08 | 2010-11-17 | 中国科学院生态环境研究中心 | Handheld gas chromatograph |
| CN102043027B (en) * | 2010-10-26 | 2013-04-10 | 上海烟草集团有限责任公司 | Method for evaluating absorbing performance of cigarette filter absorbing agent and testing system thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20030108448A1 (en) * | 2001-12-10 | 2003-06-12 | Sacks Richard Douglas | Pulsed carrier gas flow modulation for selectivity enhancements with gas chromatography using series-coupled column ensembles |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590389A (en) * | 2012-02-27 | 2012-07-18 | 上海烟草集团有限责任公司 | Gas phase chromatograph with dual detectors |
| CN102735776A (en) * | 2012-07-03 | 2012-10-17 | 中昊晨光化工研究院 | Gas chromatographic separation system and application thereof, and method for detecting trace impurities in tetrafluoroethylene |
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| JP5250164B2 (en) | 2013-07-31 |
| US20130192340A1 (en) | 2013-08-01 |
| WO2012139340A1 (en) | 2012-10-18 |
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